US6309702B1 - Process for the production of improved boron coatings - Google Patents

Process for the production of improved boron coatings Download PDF

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US6309702B1
US6309702B1 US09/382,054 US38205499A US6309702B1 US 6309702 B1 US6309702 B1 US 6309702B1 US 38205499 A US38205499 A US 38205499A US 6309702 B1 US6309702 B1 US 6309702B1
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substrate
gas
boron
chamber
heating
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Raymond J. Suplinskas
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Specialty Materials Inc
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Textron Systems Corp
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Priority to US09/945,986 priority patent/US6521291B2/en
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Priority to US10/361,130 priority patent/US6756122B2/en
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5001—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with carbon or carbonisable materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/28—Deposition of only one other non-metal element
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S427/00—Coating processes
    • Y10S427/10—Chemical vapor infiltration, i.e. CVI
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/249921—Web or sheet containing structurally defined element or component
    • Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/30—Self-sustaining carbon mass or layer with impregnant or other layer

Definitions

  • Boron coatings on graphite substrates have many useful applications. With its thermal and chemical stability, boron can be employed in the ion sources of ion implantation machines used in the manufacture of semiconductor devices. Particularly in the case of boron ion implantation, a boron or boron-coated ion source is capable of providing higher beam current, higher beam purity and lower erosion rates than ion sources made of refractory metals such as tungsten or molybdenum. Other components in ion implantation machines, such as beam dumps, could also advantageously be made of boron or boron-coated materials. Other applications occur in nuclear devices where the high temperature stability and large neutron cross-section of boron can be used in shielding and in reactor walls.
  • Pure elemental boron is difficult to fabricate into such components by ordinary means.
  • the pure element is refractory and brittle, and near its melting point, boron has a very high vapor pressure.
  • the usual metal fabrication process of casting and machining cannot be used to fabricate components.
  • ceramic processing techniques be applied readily. Hot-pressing of boron powders to fabricate plates or shapes leads to high residual stresses which result in immediate or eventual failure during use.
  • Chemical vapor deposition is a practical method for forming boron coatings.
  • the manufacturing of CVD boron fibers is a well-known technology. Boron-coated fibers prepared by CVD processes are in widespread use. For example, a description of one process of application of a boron-based refractory metal on a silicon carbide filament is taught by U.S. Pat. No. 4,481,257, which patent is incorporated herein by reference.
  • a small diameter substrate wire typically tungsten or carbon, is heated in the presence of a boron halide and hydrogen. The boron halide is reduced and elemental boron deposits on the substrate.
  • Tungsten substrate wires are typically in the range of 10 to 12 microns in diameter, while carbon substrate wires are typically somewhat thicker in the range of 25 to 50 microns in diameter.
  • the resulting boron-coated fibers are in the range of 100 to 200 microns in diameter.
  • the components required for semiconductor applications have dimensions much larger than those of the fibers, for example in the range of 5 to 15 centimeters.
  • Application of fiber CVD technology to the formation of boron coatings on these substrates does not provide suitable results.
  • the boron coatings exhibit multiple cracks and tend to spall off the substrates. A major reason for this is a mismatch of coefficients of thermal expansion (CTE) between the substrate and the boron coating.
  • CTE coefficients of thermal expansion
  • the coatings are deposited at temperatures in excess of 1000° C. Upon cooling to ambient temperature, the differential shrinkage between the substrate and coating results in stresses which crack the coating and/or result in lack of adhesion (i.e. produce a fracture at the interface between the coating and the substrate).
  • thermal stresses can be minimized by selecting a substrate material which has the same thermal expansion characteristics as those of boron.
  • the surface of a graphite or comparable substrate that is to be coated with boron is first densified with carbon to reduce surface porosity while still retaining sufficient surface texture to enhance the adherence of the subsequently applied boron coating.
  • a relatively porous graphite substrate is immersed in a liquid hydrocarbon. While under immersion, the substrate is heated by suitable means to a temperature above the decomposition temperature of the hydrocarbon. This creates a temperature gradient through the substrate, the hottest portion being in the body interior, and the coolest being at the surface of the substrate. As hydrocarbon vapors diffuse into the substrate interior through the pores, they reach the hottest portion in the interior of the body, where the temperature exceeds the decomposition temperature of the hydrocarbon. At this temperature, the vapors decompose and deposit solid carbon in the pores. The resultant substrate is thereby densified and prepared for subsequent boron deposition.
  • chemical vapor infiltration of the substrate pores with a gaseous hydrocarbon is employed to prepare the substrate surface by at least partially filling the surface porosity, while preserving adequate surface texture for good adherence of a subsequently applied boron coating.
  • excellent substrate bonding surfaces are achievable with both embodiments of this invention.
  • FIG. 1 is a schematic illustration of an apparatus suitable for carrying out the rapid densification embodiment of this invention.
  • FIG. 2 is a schematic illustration of an apparatus suitable for carrying out the chemical vapor infiltration embodiment of this invention.
  • This invention is directed to improved methods for preparing a generally porous substrate or preform for subsequent surface coating with boron.
  • Graphite substrates prepared for example by hot pressing graphite powders into the desired shape and size, are preferred substrates for this invention because graphite is not reactive with boron and has substantially the same coefficient of thermal expansion.
  • Other materials having comparable properties, however, would also be useful as substrates in accordance with this invention. Because substrates formed from such materials would likely be made by hot pressing powders or similar techniques, the resulting substrates would have a degree of porosity. Accordingly, it is believed that all such substrates could benefit from the porosity-reduction treatment processes of this invention where the substrate surface is to be subsequently coated with boron.
  • a porous substrate is immersed in a liquid hydrocarbon, for example cyclohexane, and, while immersed, is heated by suitable means to a temperature above the decomposition (and boiling) temperature of the hydrocarbon. Heat loss at the surface of the substrate to the surrounding rapidly boiling liquid creates a steep temperature gradient through the substrate with the maximum temperature at the interior of the substrate body and the minimum temperature at the surface of the substrate. Vapors of the hydrocarbon diffuse into the substrate interior through the pores.
  • a liquid hydrocarbon for example cyclohexane
  • the hydrocarbon vapors When the hydrocarbon vapors reach a depth into the substrate at which the temperature is sufficiently high, the vapors decompose resulting in the deposition of solid carbon, which at least partially fills the pores of the substrate, and the production of gaseous byproducts.
  • the depth at which this hydrocarbon decomposition temperature is achieved can be controlled by varying the power input to the substrate.
  • Rapid densification technology is generally known in the art, although it has not previously been utilized for the specific purpose of improving the quality, durability, and coating adhesion of a boron-coated article, specifically a boron-coated graphite substrate.
  • rapid densification of a carbon preform by immersion in cyclohexane while the preform is heated to at least the decomposition temperature of cyclohexane is described in U.S. Pat. No. 4,472,454, which is incorporated herein by reference.
  • More recent applications of the rapid densification technique are described in U.S. Pat. Nos. 5,389,152 (Thurston et al.); 5,397,595 (Carroll et al.); and 5,733,611 (Thurston et al.), each of which is incorporated herein by reference.
  • the determining factor in the rapid densification process of the present invention is the heat loss at the substrate surface
  • a useful measure of the process conditions is the total power input divided by the surface area of the substrate. For example, it has been found that surface treatment by the RDTM rapid densification process of this invention for a typical graphite substrate at a power level of 350 W/sq. in. produced the desired effect while undesirable results were obtained at power levels of about 50 W/sq. in. above or below this level.
  • FIG. 1 shows a reaction vessel 1 fitted with a cover 10 to contain hydrocarbon liquid 60 and hydrocarbon and other vapors in the region 12 above the surface 70 of liquid 60 .
  • Electrode posts 20 and 22 pass through cover 10 and extend into the interior of reactor 1 and into liquid 60 .
  • posts 20 and 22 are connected respectively to electrical contacts 40 and 42 which provide mechanical support for as well as electrical contact to the porous article 50 which is to be densified in accordance with the present invention.
  • Reactor 1 contains sufficient hydrocarbon liquid 60 to completely immerse article 50 therein.
  • Cover 10 includes an outlet 80 for hydrocarbon and other vapors escaping from the interior region 12 of reactor 1 .
  • Outlet 80 connects to a reflux condenser 90 to condense hydrocarbon vapor that escapes from region 12 .
  • Condensed liquid hydrocarbon is returned to reactor 1 through outlet 80 while non-condensible reaction products and uncondensed hydrocarbon vapors are exhausted from the system through vent 92 .
  • Example 1 below utilized an apparatus substantially comparable to that illustrated in FIG. 1 for carrying out comparative tests to demonstrate the superiority of boron-coated graphite substrates when the substrates have been treated in accordance with the rapid densification embodiment of this invention prior to being coated with boron.
  • Substrate samples of DFP-2 grade graphite, purchased from POCO Graphite Inc. were machined to form 5.64′′ ⁇ 0.50′′ ⁇ 0.092′′ coupons. The coupons were clamped between copper electrodes and submerged in cyclohexane contained in a three liter reaction vessel which was equipped with a reflux condenser.
  • the reactors were then purged with 5L/minute of hydrogen while heating the coupons to a temperature of 1300 ⁇ 10° C.
  • a flow of 3.4 L/minute of boron trichloride was added to the hydrogen flow into the reactor to vapor deposit boron on the surfaces of the graphite coupons. Boron deposit was then continued for about 30 minutes to form a boron coating having a thickness of about 125 microns.
  • the boron trichloride flow was then removed from the hydrogen flow into the reactor and the coupons were then slowly cooled over a period of 40 minutes by gradually reducing the current flow through the coupons.
  • CVI chemical vapor infiltration
  • a gaseous hydrocarbon inside the pores by application of heat.
  • Hydrocarbons useful for the CVI embodiment of this invention include methane, benzene, acetylene and others.
  • FIG. 2 shows a reactor vessel 100 , preferably a quartz tube, sealed at its two ends with flanges 102 and 104 respectively.
  • Flange 102 includes a gas inlet 106 connected to metered sources of a suitable hydrocarbon such as methane, and an inert gas such as argon.
  • Flange 104 includes an exhaust or gas outlet 108 .
  • a gas or mixture of gases can be flowed into reactor 100 through inlet 106 , through the interior 112 of reactor 100 , and out through outlet 108 .
  • Water-cooled electrode posts 120 and 122 pass through one of flanges 102 or 104 (shown as flange 102 in FIG. 2) and extend into the interior 112 of reactor 100 . Inside reactor 100 , posts 120 and 122 are connected respectively to clamp/electrical contacts 140 and 142 which provide mechanical support for as well as electrical contact to the porous article 150 which is to be densified in accordance with the present invention.
  • Electrodes 120 and 122 external of reactor 100 provide connections to a supply of electrical power (not shown).
  • chemical vapor infiltration is carried out on article 150 by applying electrical power to electrode posts 120 and 122 at an appropriate level to heat article 150 to the desired temperature for a sufficient period of time while flowing a suitable hydrocarbon gas through reactor 100 and past article 150 .
  • the supply of methane (or other hydrocarbon gas) or a hydrocarbon/inert gas mixture is stopped and the reactor 100 is swept with a cleansing gas such as nitrogen, or otherwise purged by means of a vacuum pump.
  • a flow of boron trichloride and hydrogen into reactor 100 can be started to deposit a high-quality boron coating on the prepared surface of article 150 by chemical vapor deposition.
  • the hydrocarbon/inert gas flow may be purged by the boron trichloride/hydrogen gas flow itself. It will be apparent that different component elements inside and outside reactor 100 would be utilized where article 150 is heated by induction or radiant heating or by some other such heating means than the electrical resistance heating illustrated in FIG. 2 .

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Vapour Deposition (AREA)
  • Carbon And Carbon Compounds (AREA)
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US09/382,054 1998-08-31 1999-08-24 Process for the production of improved boron coatings Expired - Fee Related US6309702B1 (en)

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US09/945,986 US6521291B2 (en) 1998-08-31 2001-09-04 Process for the production of improved boron coatings
US10/361,130 US6756122B2 (en) 1998-08-31 2003-02-07 Process for the production of improved boron coatings

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US20200232092A1 (en) * 2015-03-23 2020-07-23 Goodrich Corporation Systems and methods for chemical vapor infiltration and densification of porous substrates

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EP1984096B1 (en) * 2006-01-30 2014-04-30 Advanced Technology Materials, Inc. A method of increasing the loading capacity of a porous carbon adsorbent
JP2013234369A (ja) * 2012-05-10 2013-11-21 Shin-Etsu Chemical Co Ltd グラファイト材に熱分解窒化ほう素をコーティングする方法及びその方法によって得られた被覆物
EP3473746B1 (en) * 2017-10-05 2021-12-01 Goodrich Corporation Systems and methods for chemical vapor infiltration and densification of porous substrates
WO2022197172A1 (ru) * 2021-03-18 2022-09-22 Автономная Организация Образования "Назарбаев Университет" Пористый графитовый источник жидкого прекурсора углерода

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AU5581799A (en) 2000-03-21
KR20010079710A (ko) 2001-08-22
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